Dichloromethane → 7-Fluoro-5-methyl-2-(4-methyl-3-oxopiperazin-1-yl)-6-phenyl-1,3-benzoxazole-4-carbonitrile

HRID 17474노트

반응식

HRID 17474 반응식
C(N(C(C)C)CC)(C)C.Cl.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][C:13]1=[O:18].ClCCl.Cl[C:23]1[O:24][C:25]2[C:26](=[C:28]([C:40]#[N:41])[C:29]([CH3:39])=[C:30]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:31]=2[F:32])[N:27]=1>C(Cl)(Cl)Cl>[F:32][C:31]1[C:30]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[C:29]([CH3:39])[C:28]([C:40]#[N:41])=[C:26]2[C:25]=1[O:24][C:23]([N:15]1[CH2:16][CH2:17][N:12]([CH3:11])[C:13](=[O:18])[CH2:14]1)=[N:27]2

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 81531DiisopropylethylamineHCID 170607661-Methylpiperazin-2-one--hydrogen chloride (1/1)HCID 510414292-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

생성물 1

HCID 685845617-Fluoro-5-methyl-2-(4-methyl-3-oxopiperazin-1-yl)-6-phenyl-1,3-benzoxazole-4-carbonitrile수율 99.9%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Diisopropylethylamine (232 μl, 1.36 mmol) and 1-methylpiperazin-2-one hydrochloride (103 mg, 0-682 mmol) were added to a dichloromethane (6 ml) solution of 2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (163 mg, 0.569 mmol), followed by stirring at room temperature for 30 minutes. Chloroform (50 ml) was added to the reaction liquid, followed by washing with saturated brine (50 ml). After drying over anhydrous sodium sulfate and concentration under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent, chloroform:methanol=20:1) to obtain the entitled compound (207 mg, 99.9%) as a colorless solid.

후처리

  1. washby washing with saturated brine (50 ml)
  2. dry with materialAfter drying over anhydrous sodium sulfate and concentration under reduced pressure
  3. customthe resulting residue was purified by silica gel column chromatography (eluent, chloroform:methanol=20:1)

출처 및 근거

ORD 기록
ord-8aee05eaa86143319375b494e6912907
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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